CN113773223B - Method for purifying 2-amino-4-acetamino anisole by precipitation method - Google Patents
Method for purifying 2-amino-4-acetamino anisole by precipitation method Download PDFInfo
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- CN113773223B CN113773223B CN202111066721.9A CN202111066721A CN113773223B CN 113773223 B CN113773223 B CN 113773223B CN 202111066721 A CN202111066721 A CN 202111066721A CN 113773223 B CN113773223 B CN 113773223B
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Abstract
The invention belongs to the technical field of fine chemical engineering, and particularly relates to a method for purifying 2-amino-4-acetamido anisole by a precipitation method. Adding a precipitant into the 2-amino-4-acetamidoanisole production mother liquor, filtering, resolving the obtained precipitate to obtain a water phase and an organic phase, regulating the pH value of the water phase, drying to obtain 2-amino-4-acetamidoanisole, distilling the organic phase, and recovering the obtained organic solvent, wherein the obtained precipitant can be reused. The method adopts a precipitation method to purify the 2-amino-4-acetaminophen, has the advantages of low energy consumption and high reaction efficiency, and can realize the purpose of high selectivity to obtain the 2-amino-4-acetaminophen with high purity and high yield; and the operation is simple, and the economic value and the environmental benefit are obvious.
Description
Technical Field
The invention belongs to the technical field of fine chemical engineering, and particularly relates to a method for purifying 2-amino-4-acetamido anisole by a precipitation method.
Background
2-amino-4-acetamido anisole (commonly called as reducing substance) is a key intermediate in the disperse dye industry, and can be used for producing more than ten dyes such as disperse blue, disperse violet, disperse yellow and the like subsequently. In the dye industry, the annual demand of the dye reaches more than 30 ten thousand tons, and the dye has important economic value. The 2-amino-4-acetamido anisole synthesis process mainly comprises two steps, wherein the traditional synthesis process takes paranitrochlorobenzene as a raw material, and the paraacetamido anisole is obtained through etherification, hydrogenation reduction and acetylation reaction, and then the target product is obtained through nitration and hydrogenation reduction reaction. The specific equation is as follows:
the traditional synthesis process is a very mature process, and the byproduct 2, 4-diacetylanisole is hardly generated in the synthesis process, but the process has a plurality of problems, such as low yield, complex production steps, and the like, and a large amount of wastewater, waste residues and the like polluting the environment are generated. The new synthesis process is to synthesize the target product by etherification reaction, hydrogenation reduction reaction and acetylation reaction with 2, 4-dinitrochlorobenzene as initial material. The specific equation is as follows:
the 2-amino-4-acetamino anisole improves the industrial safety coefficient in the production and preparation of the new process, reduces the industrial cost, but generates a small amount of 2, 4-diacetyl anisole byproducts in the process of synthesizing the 2-amino-4-acetamino anisole by the new process, and can obtain the 2-amino-4-acetamino anisole with higher purity by a purification method.
Xu Wenlin, duan Yuhui, liu Xueqian. Process for preparing 2-amino-4-acetamidoanisole [ P ]. Jiangsu: CN1861577A,2006-11-15 reports that 2-amino-4-acetaminophen ether is purified by crystallization separation and refining method, 2-amino-4-acetaminophen ether crude product is put into a crystallization kettle of a crystallization separator for evaporation and crystallization separation and refining, methanol is added as solvent, the dosage ratio of 2-amino-4-acetaminophen ether to methanol is 100g:150mL, the temperature is raised to reflux temperature, the operation temperature is kept at 20 ℃ to methanol reflux temperature, the operation pressure is 0.2MPa, the temperature is kept for 30min under reflux condition, then the temperature is slowly reduced to 20 ℃, and the method does not refer to the purity and yield after purification.
Luo Zhijiang, liu Jian, shen Dongsheng, yang Liwen, lin Yuan New Process for synthesizing 3-amino-4-methoxyacetanilide [ J ]. Dye industry, 2001 (05): 28-29+22. 3-amino-4-methoxyacetanilide is reported to be purified by adjusting the pH to 3-4 by adding concentrated hydrochloric acid after the selective acylation reaction is finished, a large amount of white precipitate is precipitated, filtered, and washed twice with methanol. The obtained precipitate is dissolved in 150mL of water, the pH value is regulated to 9-10 by dilute sodium hydroxide, and 3-amino-4-methoxy acetanilide can be separated out, the yield is 86%, and the purity is 98%.
At present, the method for purifying 2-amino-4-acetaminophen from 2-amino-4-acetaminophen production mother liquor mainly adopts a recrystallization method, but the recrystallization method for purifying 2-amino-4-acetaminophen has a plurality of problems: (1) It is difficult to select a suitable recrystallization solvent, resulting in low purity; (2) The recrystallization needs to be heated by reflux, cooled again and crystallized out, and a large amount of 2-amino-4-acetaminophen ether still remains in the filtrate, so that the yield is reduced.
Therefore, it is needed to provide a purification method of 2-amino-4-acetamido anisole, which improves the product yield, reduces the existence of byproducts, saves energy consumption and is more environment-friendly.
Disclosure of Invention
The invention aims to provide a method for purifying 2-amino-4-acetaminophen ether by a precipitation method, which is characterized in that a precipitator is added into a mother liquor for producing 2-amino-4-acetaminophen ether, and then the precipitate is resolved, so that the 2-amino-4-acetaminophen ether can be effectively purified, and the product has high yield and high purity.
The technical scheme adopted for solving the technical problems is as follows:
according to the method for purifying 2-amino-4-acetaminophen by using the precipitation method, a precipitator is added into a mother liquor for producing 2-amino-4-acetaminophen, the obtained precipitate is filtered, a water phase and an organic phase are obtained after the analysis, and the water phase is subjected to pH value adjustment and drying to obtain the 2-amino-4-acetaminophen.
Wherein:
the 2-amino-4-acetamido anisole production mother liquor contains 2-amino-4-acetamido anisole and 2, 4-diacetylamido anisole; wherein the content of 2-amino-4-acetamidoanisole is 93-96wt.%, and the content of 2, 4-diacetylaminoanisole is 4-7wt.%; the preparation method comprises the steps of taking 2, 4-dinitroanisole as a raw material and ethyl acetate as a solvent, and carrying out hydrogenation reduction reaction and selective acylation reaction to obtain the catalyst:
taking 2, 4-dinitroanisole as a raw material, ethyl acetate as a reaction solvent, adding 5% Pd/C as a catalyst, and introducing hydrogen to react at the temperature of 75-80 ℃ and the pressure of 2-3MPa to obtain 2, 4-diaminoanisole reaction liquid; acetic anhydride with the molar ratio of 1:1-1.1 is added into the 2, 4-diaminoanisole reaction liquid to carry out selective acylation, thus obtaining the 2-amino-4-acetamido anisole production mother liquid.
The general formula of the precipitant is as follows:
wherein: r is R 1 、R 2 ＝-H、-CH 3 、-OH、-OCH 3 、-Cl、-Br、-NO 2 or-NH 2 。
The mol ratio of the precipitant to the 2-amino-4-acetaminophen in the 2-amino-4-acetaminophen production mother liquid is 1-5:1.
Resolving by adopting a mixed solution of an aqueous acid solution and an organic solvent; the acid is hydrochloric acid, sulfuric acid or phosphoric acid; the organic solvent is water-insoluble chlorinated hydrocarbon, ester or toluene, preferably dichloromethane, chloroform, ethyl acetate, butyl acetate or toluene.
The concentration of the aqueous solution of the acid is 0.4-2mol/L, the mol ratio of the 2-amino-4-acetamido anisole to the acid in the 2-amino-4-acetamido anisole production mother solution is 1:1-5, and the volume ratio of the organic solvent to the aqueous solution of the acid is 1:1-3.
The analysis temperature is 10-40 ℃ and the analysis time is 1-2h.
And regulating the pH value to 5-9 by adopting a pH regulator. The pH regulator is sodium hydroxide solution, sodium carbonate solution or sodium bicarbonate solution; the concentration of the pH regulator is 0.5-30wt.%.
And distilling the organic phase to obtain a solvent, and recovering the solvent to obtain the precipitant for recycling. The drying is spray drying.
The invention takes acetophenone as a precipitator for purifying 2-amino-4-acetamido anisole production mother liquor, and the reaction process is as follows:
the beneficial effects of the invention are as follows:
according to the invention, the characteristic of Lewis base of amino in 2-amino-4-acetamido anisole is utilized, so that Schiff base structure can be formed with ketone groups in the precipitant, and precipitation is generated, thereby realizing solid-liquid separation of 2-amino-4-acetamido anisole and mother liquor; then the obtained solid precipitate is subjected to acid precipitation hydrolysis by using an aqueous solution of acid and an organic solvent, and the precipitant has hydrophobicity and can be better dissolved in the organic solvent, so that the precipitant is promoted to enter an organic phase, the acid precipitation hydrolysis is facilitated, the organic phase can be recycled, and 2-amino-4-acetaminophen enters the aqueous phase; the byproduct 2, 4-diacetylanisole cannot react with the precipitant due to no amino group, so that no precipitate is generated, the purification and separation of the main product and the byproduct are realized, the purpose of high selectivity is achieved, and the 2-amino-4-acetamidoanisole with higher purity is obtained.
Compared with a recrystallization method, the precipitation method is carried out at normal temperature through chemical reaction, and the recrystallization method needs to be heated to reflux temperature, so that the temperature is higher; the precipitation method enables the main product to react with the precipitant to separate out precipitate through chemical reaction, the byproducts are kept in the mother liquor, the yield of the 2-amino-4-acetaminophen is greatly improved, the recrystallization method needs cooling to separate out, and part of the 2-amino-4-acetaminophen still remains in the filtrate, so that the influence on the yield of the finished product is great; the organic phase and the aqueous phase can be recycled by using a precipitation method.
The method adopts a precipitation method to purify the 2-amino-4-acetaminophen ether, has the advantages of low energy consumption and high reaction efficiency, can realize the purpose of high selectivity, and obtains the 2-amino-4-acetaminophen ether with higher purity and higher yield; and the operation is simple, and the economic value and the environmental benefit are obvious.
Detailed Description
The invention is further described below with reference to examples.
Example 1
300g of 2, 4-dinitroanisole is weighed as a raw material, ethyl acetate is used as a reaction solvent, 5% Pd/C is added as a catalyst, and hydrogen is introduced to react at the temperature of 75 ℃ and the pressure of 2MPa to obtain a 2, 4-diaminoanisole reaction solution; acetic anhydride with the raw material molar ratio of 1:1 is added into the 2, 4-diaminoanisole reaction liquid for selective acylation, so as to obtain 2-amino-4-acetaminophen production mother liquid, wherein the content of 2-amino-4-acetaminophen is 95.5 wt%, the content of 2, 4-diacetylaminoanisole is 4.0 wt%, and the balance is impurities.
Taking 500g of the mother liquor for producing 2-amino-4-acetamidoanisole, adding acetophenone at normal temperature, wherein the molar ratio of acetophenone to 2-amino-4-acetamidoanisole in the mother liquor for producing 2-amino-4-acetamidoanisole is 1:1, separating out solid precipitate in the mother liquor, filtering out the solid precipitate by using a Buchner funnel, carrying out acid precipitation hydrolysis on the precipitate, adding a mixed solution of dilute hydrochloric acid and toluene (the concentration of the dilute hydrochloric acid solution is 2mol/L, the volume consumption is 2.65L, the consumption of toluene is 2.5L), controlling the molar ratio of 2-amino-4-acetamidoanisole to hydrochloric acid to be 1:2, stirring for 1h at 30 ℃, transferring to a separating funnel, standing for 20min to generate layering, wherein the upper layer is organic phase toluene, the lower layer is water phase, recovering the organic solvent by distillation, recycling the obtained precipitant by using a high-performance liquid chromatography method, and obtaining a water phase sample, wherein the purity of the 2-amino-4-acetamidoanisole reaches 98.8%, the water phase is 10 wt% sodium hydroxide, the pH value is adjusted to be 1:2, and the pure amino-4-acetamidoanisole is dried to obtain the pure product, and the pure amino-4.464 is calculated to be 1.96 g.
Example 2
500g of mother liquor for producing 2-amino-4-acetamidoanisole in example 1 is taken, propiophenone is added at normal temperature, the molar ratio of the propiophenone to the 2-amino-4-acetamidoanisole in the mother liquor for producing 2-amino-4-acetamidoanisole is 1:1, at this time, solid precipitates are separated out from the mother liquor, the solid precipitates are filtered out by a Buchner funnel, the precipitates are subjected to acid hydrolysis, a mixed solution of dilute sulfuric acid and ethyl acetate (the concentration of the dilute sulfuric acid solution is 0.8mol/L, the volume consumption is 3.31L, the consumption of the ethyl acetate is 2L), the molar ratio of the 2-amino-4-acetamidoanisole to sulfuric acid is controlled to be 1:1, the mixture is stirred for 1h at 30 ℃, the mixture is transferred to a separating funnel for standing for 20min, the mixture is layered, the upper layer is organic phase ethyl acetate, the lower layer is aqueous phase, the organic phase is recovered by distillation, the obtained precipitant can be repeatedly used, the obtained aqueous phase is sampled and is detected by a high performance liquid chromatography method, the result shows that the purity of the 2-amino-4-acetamidoanisole reaches 98.4%, the purity of the aqueous phase reaches 10 wt% and the pure pH value of 10 to be adjusted to be 3.95.95%, and the pure acetamidoanisole is obtained by spraying the pure solution, and the pure pH value is calculated to be 3.95, and the pure product is calculated to be 3.95, and the yield is calculated to be 3.95.
Example 3
Taking 500g of 2-amino-4-acetaminophen ether production mother liquor in example 1, adding acetophenone at normal temperature, wherein the molar ratio of acetophenone to 2-amino-4-acetaminophen ether in the 2-amino-4-acetaminophen ether production mother liquor is 1:1, separating out solid precipitate in the mother liquor, filtering out the solid precipitate by using a Buchner funnel, carrying out acid separation hydrolysis on the precipitate, adding a mixed solution of dilute hydrochloric acid and ethyl acetate (the concentration of the dilute hydrochloric acid solution is 1mol/L, the volume consumption is 2.65L, and the consumption of ethyl acetate is 2L), controlling the molar ratio of 2-amino-4-acetaminophen ether to hydrochloric acid to be 1:1, stirring for 1h at 30 ℃, transferring to a separating funnel, standing for 20min to generate layering, wherein the upper layer is organic phase ethyl acetate, the lower layer is water phase, and the organic solvent is recovered by distillation, so that the obtained precipitant can be reused; the obtained aqueous phase was sampled and examined by high performance liquid chromatography, and the result showed that the purity of 2-amino-4-acetamidoanisole reached 99.3%, the pH of the aqueous phase was adjusted to neutral with 10wt.% sodium hydroxide solution, and spray-drying was carried out to obtain 465.9g of pure solid product 2-amino-4-acetamidoanisole, the yield of which was calculated to be 96.9%.
Example 4
Taking 500g of 2-amino-4-acetamido anisole production mother liquor in example 1, adding diphenyl ketone at normal temperature, wherein the molar ratio of diphenyl ketone to 2-amino-4-acetamido anisole in the 2-amino-4-acetamido anisole production mother liquor is 3:1, separating out solid precipitate in the mother liquor, filtering out the solid precipitate by using a Buchner funnel, carrying out acid separation hydrolysis on the precipitate, adding a mixed solution of dilute hydrochloric acid and dichloromethane (the concentration of the dilute hydrochloric acid solution is 1.5mol/L, the volume consumption is 3.53L, and the consumption of dichloromethane is 1.7L), controlling the molar ratio of 2-amino-4-acetamido anisole and hydrochloric acid to be 1:2, stirring for 1h at 30 ℃, transferring to a separating funnel, standing for 20min to generate layering, wherein the upper layer is water phase, the lower layer is organic phase dichloromethane, and the organic phase is recovered by distillation, so that the obtained precipitant can be reused; the obtained aqueous phase was sampled and examined by high performance liquid chromatography, and the result showed that the purity of 2-amino-4-acetamidoanisole was 98.8%, the pH of the aqueous phase was adjusted to 9 with 10wt.% sodium hydroxide solution, and spray-drying was performed to obtain 465.9g of pure solid product 2-amino-4-acetamidoanisole, the yield of which was calculated to be 96.4%.
Example 5
Taking 500g of 2-amino-4-acetaminophen ether production mother liquor in example 1, adding acetophenone at normal temperature, wherein the molar ratio of acetophenone to 2-amino-4-acetaminophen ether in the 2-amino-4-acetaminophen ether production mother liquor is 2:1, separating out solid precipitate in the mother liquor, filtering out the solid precipitate by using a Buchner funnel, carrying out acid separation hydrolysis on the precipitate, adding a mixed solution of dilute hydrochloric acid and ethyl acetate (the concentration of the dilute hydrochloric acid solution is 1.5mol/L, the volume consumption is 5.3L, and the consumption of ethyl acetate is 3.5L), controlling the molar ratio of 2-amino-4-acetaminophen ether to hydrochloric acid to be 1:3, stirring for 1h at 30 ℃, moving to a separating funnel, standing for 20min to generate layering, wherein the upper layer is organic phase ethyl acetate, the lower layer is water phase, and the organic phase is distilled to recover the organic solvent, so that the obtained precipitant can be reused; the obtained aqueous phase was sampled and examined by high performance liquid chromatography, and the result showed that the purity of 2-amino-4-acetamidoanisole was 98.5%, the pH value of the aqueous phase was adjusted to be neutral by 10wt.% sodium hydroxide solution, and 462.1g of pure solid product 2-amino-4-acetamidoanisole was obtained by spray drying, and the yield was calculated to be 95.3%.
Example 6
Taking 500g of 2-amino-4-acetaminophen ether production mother liquor in example 1, adding acetophenone at normal temperature, wherein the molar ratio of acetophenone to 2-amino-4-acetaminophen ether in the 2-amino-4-acetaminophen ether production mother liquor is 5:1, separating out solid precipitate in the mother liquor, filtering out the solid precipitate by using a Buchner funnel, carrying out acid separation hydrolysis on the precipitate, adding a mixed solution of dilute hydrochloric acid and butyl acetate (the concentration of the dilute hydrochloric acid solution is 2mol/L, the volume consumption is 5.3L, and the consumption of butyl acetate is 2.5L), controlling the molar ratio of 2-amino-4-acetaminophen ether to hydrochloric acid to be 1:4, stirring for 1h at 30 ℃, transferring to a separating funnel, standing for 20min to generate layering, wherein the upper layer is organic phase butyl acetate, the lower layer is water phase, and the organic phase is recovered by distillation, so that the obtained precipitant can be reused; the obtained aqueous phase was sampled and examined by high performance liquid chromatography, and the result showed that the purity of 2-amino-4-acetamidoanisole was 98.5%, the pH value of the aqueous phase was adjusted to neutral by 10wt.% sodium hydroxide solution, and spray-drying was carried out to obtain 464.2g of pure solid product 2-amino-4-acetamidoanisole, the yield of which was calculated to be 95.8%.
Example 7
Taking 500g of 2-amino-4-acetaminophen ether production mother liquor in example 1, adding dicyclohexylketone at normal temperature, wherein the molar ratio of dicyclohexylketone to 2-amino-4-acetaminophen ether in the 2-amino-4-acetaminophen ether production mother liquor is 3:1, separating out solid precipitate in the mother liquor at the moment, filtering out the solid precipitate by using a Buchner funnel, carrying out acid precipitation hydrolysis on the precipitate, adding a mixed solution of dilute hydrochloric acid and chloroform (the concentration of the dilute hydrochloric acid solution is 1.2mol/L, the volume dosage is 4.42L, the dosage of chloroform is 2L), controlling the molar ratio of 2-amino-4-acetaminophen ether to hydrochloric acid to be 1:2, stirring for 2h at 20 ℃, transferring to a separating funnel, standing for 20min to generate layering, wherein the upper layer is aqueous phase, the lower layer is organic phase chloroform, and the organic phase is distilled to recover the organic solvent, so that the obtained precipitant can be reused; the obtained aqueous phase was sampled and examined by high performance liquid chromatography, and the result showed that the purity of 2-amino-4-acetamidoanisole was 98.6%, the pH value of the aqueous phase was adjusted to neutral by 10wt.% sodium carbonate solution, and spray-drying was carried out to obtain 466.5g of pure solid product 2-amino-4-acetamidoanisole, the yield of which was calculated to be 96.3%.
Example 8
Taking 500g of 2-amino-4-acetaminophen ether production mother liquor in example 1, adding cyclohexyl ethyl ketone at normal temperature, wherein the molar ratio of the cyclohexyl ethyl ketone to the 2-amino-4-acetaminophen ether in the 2-amino-4-acetaminophen ether production mother liquor is 3:1, separating out solid precipitate in the mother liquor, filtering the solid precipitate by using a Buchner funnel, carrying out acid precipitation hydrolysis on the precipitate, adding a mixed solution of dilute hydrochloric acid and ethyl acetate (the concentration of a dilute hydrochloric acid solution is 0.4mol/L, the volume dosage is 6.63L, the dosage of ethyl acetate is 2.21L), controlling the molar ratio of the 2-amino-4-acetaminophen ether to hydrochloric acid to be 1:1, stirring for 2h at 20 ℃, moving to a separating funnel, standing for 20min to generate layering, wherein the upper layer is organic phase ethyl acetate, the lower layer is aqueous phase, and the organic phase is recovered by distillation, so that the obtained precipitant can be reused; the obtained aqueous phase was sampled and examined by high performance liquid chromatography, and the result showed that the purity of 2-amino-4-acetamidoanisole was 98.9%, the pH of the aqueous phase was adjusted to neutral with 10wt.% sodium carbonate solution, and spray-drying was performed to obtain 463.2g of pure solid product 2-amino-4-acetamidoanisole, the yield of which was calculated to be 95.9%.
Comparative example 1
500g of the mother liquor for producing 2-amino-4-acetaminophen in example 1 was taken, the organic solvent in the mother liquor was distilled off under reduced pressure, deionized water was used as a recrystallization solvent, 800mL of deionized water was added thereto, stirring was carried out to dissolve the whole, the temperature was raised to 85 ℃ and reflux was carried out for 1 hour, after the recrystallization was completed, the crystals were cooled at room temperature, in order to precipitate the crystals more completely, the crystals were cooled and crystallized further, the precipitated solids were filtered off, dried to obtain solids, and the samples were examined by high performance liquid chromatography, and as a result, 393.8g of 2-amino-4-acetaminophen was found to have a purity of 97.0% and a calculated yield of 80%.
Claims (8)
1. A method for purifying 2-amino-4-acetamido anisole by a precipitation method is characterized in that: adding a precipitant into the mother liquor for producing 2-amino-4-acetaminophen, filtering, resolving the obtained precipitate to obtain a water phase and an organic phase, regulating the pH value of the water phase, and drying to obtain 2-amino-4-acetaminophen;
the 2-amino-4-acetamido anisole production mother liquor contains 2-amino-4-acetamido anisole and 2, 4-diacetylamido anisole; wherein the content of 2-amino-4-acetamidoanisole is 93-96wt.%, and the content of 2, 4-diacetylaminoanisole is 4-7wt.%;
the general formula of the precipitant is as follows:
；
wherein: r is R 1 、R 2 ＝-H、-CH 3 、-OH、-OCH 3 、-Cl、-Br、-NO 2 or-NH 2 。
2. The method for purifying 2-amino-4-acetamidoanisole by precipitation method according to claim 1, wherein: the mol ratio of the precipitant to the 2-amino-4-acetaminophen in the 2-amino-4-acetaminophen production mother liquid is 1-5:1.
3. The method for purifying 2-amino-4-acetamidoanisole by precipitation method according to claim 1, wherein: resolving by adopting a mixed solution of an aqueous acid solution and an organic solvent; the acid is hydrochloric acid, sulfuric acid or phosphoric acid; the organic solvent is water-insoluble chlorinated hydrocarbon, ester or toluene.
4. A method for purifying 2-amino-4-acetamidoanisole by precipitation method according to claim 3, wherein: the concentration of the aqueous solution of the acid is 0.4-2mol/L, the mol ratio of the 2-amino-4-acetamido anisole to the acid in the 2-amino-4-acetamido anisole production mother solution is 1:1-5, and the volume ratio of the organic solvent to the aqueous solution of the acid is 1:1-3; the organic solvent is dichloromethane, chloroform, ethyl acetate, butyl acetate or toluene.
5. The method for purifying 2-amino-4-acetamidoanisole by precipitation method according to claim 1, wherein: the analysis temperature is 10-40 ℃ and the analysis time is 1-2h.
6. The method for purifying 2-amino-4-acetamidoanisole by precipitation method according to claim 1, wherein: and regulating the pH value to 5-9 by adopting a pH regulator.
7. The method for purifying 2-amino-4-acetamidoanisole by precipitation method according to claim 6, wherein: the pH regulator is sodium hydroxide solution, sodium carbonate solution or sodium bicarbonate solution; the concentration of the pH regulator is 0.5-30wt.%.
8. The method for purifying 2-amino-4-acetamidoanisole by precipitation method according to claim 1, wherein: and distilling the organic phase to obtain a solvent, and recovering the solvent to obtain the precipitant for recycling.
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| CN104788334A (en) * | 2015-04-13 | 2015-07-22 | 上海综星化工科技有限公司 | Synthesis process of 2-amino-4-acetamino anisole |
| CN107746380A (en) * | 2017-11-06 | 2018-03-02 | 宁夏中盛新科技有限公司 | A kind of industrialized preparing process of the acetyl-anisidine of 2 amino 4 |
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| CN104788334A (en) * | 2015-04-13 | 2015-07-22 | 上海综星化工科技有限公司 | Synthesis process of 2-amino-4-acetamino anisole |
| CN107746380A (en) * | 2017-11-06 | 2018-03-02 | 宁夏中盛新科技有限公司 | A kind of industrialized preparing process of the acetyl-anisidine of 2 amino 4 |
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